CN102344154A - Method for preparing high-purity magnesium chloride hexahydrate from waste brine - Google Patents
Method for preparing high-purity magnesium chloride hexahydrate from waste brine Download PDFInfo
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- CN102344154A CN102344154A CN2010102447083A CN201010244708A CN102344154A CN 102344154 A CN102344154 A CN 102344154A CN 2010102447083 A CN2010102447083 A CN 2010102447083A CN 201010244708 A CN201010244708 A CN 201010244708A CN 102344154 A CN102344154 A CN 102344154A
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Abstract
The invention provides a method for removing trace impurities in magnesium chloride by using waste brine discharged in potassium chloride production as a raw material by an improved two-stage recrystallization technique. Each stage of the crystallization technique comprises the following steps: 1) free settling, 2) natural evaporation and crystallization, 3) size-grading selective recycling, 4) filtration, (5) saturated magnesium chloride solution washing and the like. By using the method, trace impurities, such as boron, sulfur, ferrum and the like, in magnesium chloride can be reduced to less than 5 ppm, and the purity of the product magnesium chloride hexahydrate is higher than 99.5%. The invention has the characteristics of low energy consumption and low cost, is simple to operate, and is applicable to refining magnesium metal, flame retardant, magnesium hydroxide or any other raw material by an electrolytic process.
Description
Invention field
The invention belongs to chemical industry and raw materials for metallurgy preparation field; Particularly adopt the method for the high-purity magnesium chloride hexahydrate of lower-cost natural recrystallization prepared, and then be used as the raw material for preparing the required anhydrous magnesium chloride with high purity of electrolytic magnesium or produce other high-purity magnesium salts products.
Technical background
China's Qinghai Chaerhan salt lakes contains abundant magnesium resource, and reserves are 4,000,000,000 tons, occupy the second place of the world, accounts for world's total reserves 1/3.At present, Qinghai Chaerhan salt lakes is arranged a large amount of useless bittern in producing the potash fertilizer process.According to incompletely statistics, ten thousand tons of the about 350-400 of the Cha Er sweat salt lake annual Repone K ultimate production in area, the useless bittern that production process need be discharged is up to the 4000-5000 ten thousand stere.This is that MAGNESIUM METAL and magnesium salts products production provide sufficient reliable raw material source.Simultaneously, Repone K production is discharged useless bittern and is had the advantages that magnesium chloride purity is high, concentration is high, and the area, salt lake has few and the weather condition that steam output is big of rainfall amount in addition, for spontaneous evaporation recrystallization purification magnesium chloride has been created condition.
The electrolytic process MAGNESIUM METAL requires very high to the Magnesium Chloride Anhydrous foreign matter content, impurity such as S, Fe, B have material impact to electrolytic cell currents efficient in the Magnesium Chloride Anhydrous.Being elevated to 50ppm like B, S content from 10ppm can cause electrolytic cell currents efficient to drop to below 65% from 85%.Therefore, this just requires that impurity such as S, Fe, B must drop to below the 10ppm in the magnesium chloride raw material.
Simultaneously, some magnesium salts chemical also have strict requirement to raw material impurity content.Like flame-proof magnesium hydroxide; Magnesium hydroxide as the flame-retardant additive use in; Because heavy metal ion such as Cr wherein, Mn, Fe have significant detrimentally affect to synthetic materials performances such as plastics, resins, thereby require content of impurities such as heavy metal Cr in the raw materials for production, Mn, Fe must be lower than 100ppm.
At present, the magnesium chloride of purifying both at home and abroad has several different methods, all more or less has some problems but be applied to bittern production magnesium chloride hexahydrate.As, patented methods such as ZL97114157.6, ZL93109924.2 are that specific aim removes sulfate radical, and can't guarantee that sulphur content reduces to below the 10ppm, and other foreign matter contents such as B, Fe are still higher; The method that CN1134917 proposes is that bittern is heated to nearly boiling point, and insulation is filtered, then evaporative crystallization.This method is owing to impurity ion content in the solution is higher, and a recrystallization is difficult to guarantee that S, Fe, B plasma all are reduced to below the 10ppm, and needs to consume significant amount of energy.
Based on the problem that exists in the above-mentioned prior art, a kind of method that can prepare high-purity Magnesium dichloride hexahydrate is sought in the present invention's expectation, preferably hopes to seek a kind of method that can under the situation that need not consume mass energy consumption, can prepare Magnesium dichloride hexahydrate.
Summary of the invention
Based on the problem that exists in the above-mentioned prior art; The present invention is from conventional recrystallizing technology; Make improvements; Through crystalline particle being selected recovery; From crystalline particle, reclaim the high crystalline particle of purity and then it is carried out treatment process such as filtration washing; Can utilize useless bittern to be the technology of the high-purity Magnesium dichloride hexahydrate of raw material production with acquisition, specific as follows:
A kind of useless bittern of discharging with Repone K production is the method for the high-purity magnesium chloride hexahydrate of raw material production, comprises the steps:
First purification phase comprises that useless bittern is successively through obtaining coarse crystallization after first settling process, first evaporation and crystal process, first crystallization selection removal process, the first filtration washing process;
Second purification phase comprises resulting coarse crystallization is dissolved once more, selected removal process, the second filtration washing process through second settling process, second evaporation and crystal process, second crystallization, obtains wet crystallization, obtains finished product behind the crystallizing and drying that will wet;
It is characterized in that; Said first crystallization selects the removal process and second crystallization to select removal process to adopt crystallization to select withdrawer to come the crystallization of selective recovery certain grain size scope; Said crystallization selects withdrawer to have following structure: the opening for feed of crystallization withdrawer is arranged on the middle and upper part; The inclination sieve plate is equipped with in the opening for feed below; Be the circulating clear liquid import below the sieve plate, discharge port is arranged at the bottom; Wait that selecting to reclaim crystallization gets into from the withdrawer middle and upper part with the slurries form; Particle diameter is stopped entering macrobead recovery approach greater than 4 millimeters crystalline particle by sieve plate, reclaims or dissolve the back once more with coarse crystallization as byproduct to get into second purification phase; Diameter overflows withdrawer less than 0.1 millimeter particle with the current overflowing liquid that makes progress, and diameter 0.1-4 mm granules is deposited to the withdrawer bottom through the inclination sieve plate, is discharged by the bottom discharge mouth, gets into filtration washing process subsequently.
Owing to all contain impurity such as similar Fe in the magnesium chloride near saturated solution of useless bittern or steam condensate preparation; Therefore preferably in above-mentioned first and/or second settling process, add sinking agent; Make foreign ion become solid precipitation earlier through sinking agent; It is agglomerating that these solid precipitations are assembled, thereby more effectively remove most of foreign ion.Sinking agent in the conventional preparation magnesium chloride crystallisation process all can adopt, but the sinking agent that more preferably uses among the present invention is one or more the aqueous solution that is selected from AG hydrochloric acid, calcium chloride, bariumchloride, sodium-chlor, yellow soda ash, sodium hydroxide, polyoxyethylene glycol, polyacrylamide, the only son's acid.The solution of sinking agent preferably adopts the deionized water configuration, more preferably adopts the configuration of distilled water or ultrapure water, can also adopt the steam condensate configuration, so that introduce foreign ion still less.Wherein, the sinking agent that in first and second settling processes, adds can be identical also can be different.
The mass percent concentration of the preferred sinking agent aqueous solution is 1-25%.The consumption of sinking agent solution can be formed variation according to raw material in the production process, quality product is regulated, and preferable amount is 0.5～1.0% (weight) of the former liquid measure of sedimentation.
Above-mentioned first evaporation and crystal process and second evaporation and crystal process can adopt this area evaporation and crystal process commonly used; But consideration from the energy efficient that reduces cost; Preferably first or second evaporation and crystal process adopts the spontaneous evaporation crystallization processes, and more preferred first and second evaporation and crystal processes all adopt the spontaneous evaporation crystallization processes.But those skilled in the art should recognize; In actual natural evaporation crystallization process; Because evaporation and crystal process is exposed in the natural environment fully; Air flows or wind can carry fine dust entering evaporative crystallization pond; So crystalline product purity purity for enclosed evaporation and crystal process is low slightly; But select recover owing to used the crystallization of foregoing ad hoc structure among the present invention; It also can remove the fine dust that air flows or wind carries when product is proposed, the specific crystallization of promptly being adopted among the present invention selects recover also can guarantee the product purity under the natural evaporation crystallization condition.
Further, the washing lotion used of the said first filtration washing process is the saturated magnesium chloride solution of steam condensate, distilled water, deionized water or the configuration of high-purity finished product magnesium chloride; The washing lotion of using in the perhaps said second filtration washing process is the saturated magnesium chloride solution of steam condensate and the configuration of high-purity finished product magnesium chloride; More preferably, the washing lotion of first, second filtration washing is the clear liquid of magnesium chloride saturated solution after sedimentation with steam condensate and finished product configuration; Preferred washing lotion consumption is the 10-30% of slurry weight.Adopt the saturated magnesium chloride solution of steam steam condensate, distilled water, deionized water or the configuration of high-purity finished product magnesium chloride to wash; Can avoid in washing process, introducing unnecessary impurity effectively; Thereby also can avoid causing the problem of product yield soybean reduction simultaneously, guarantee product gas purity and yield because of magnesium chloride is very easily water-soluble.
The coarse crystallization product that first evaporation and crystal process obtains has preferably adopted steam condensate when dissolving; Other the deionized water, distilled water or the ultrapure water that contain S, Fe, the reduction of B constituent content all can be selected, but more preferably adopt steam condensate from the consideration of cost.
Technique effect
The present invention selects the improved secondary recrystallization technology of withdrawer can remove all impurity effectively through the crystallization of using ad hoc structure; Can also make full use of simultaneously the Qinghai big weather condition of local steam output and carry out the spontaneous evaporation crystallization, greatly reduce processing cost.The product that adopts this patent method to prepare not only can satisfy dehydration and produce the anhydrous magnesium chloride with high purity requirement, also can be used for production high purity fire retardant magnesium hydroxide.
Description of drawings
Accompanying drawing 1 has provided the process flow sheet of a preferred implementation of the present invention
Accompanying drawing 2 has provided the structural representation of the crystallization selection withdrawer of ad hoc structure of the present invention
Description of reference numerals in the accompanying drawing 2: feed slurry inlet 1, overflow groove 2, sieve plate 3, circulating clear liquid import 4, macrobead reclaims mouth 5, discharge port 6.
Crystallization selects the withdrawer structure shown in accompanying drawing 2.Withdrawer opening for feed 1 is in the middle and upper part, and inclination sieve plate 3 is equipped with in opening for feed 1 below, is circulating clear liquid import 4 below the sieve plate.Wait that selecting to reclaim crystallization gets into from opening for feed with the slurries form.Particle diameter is stopped entering macrobead recovery approach 5 greater than 4 mm granules by sieve plate, and diameter gets into overflow groove 2 less than 0.1 millimeter particle with upward water flow, and diameter 0.1-4 mm granules is deposited to the withdrawer bottom through the inclination sieve plate, is discharged by bottom discharge mouth 6.
Embodiment
Below will come the present invention is set forth through a particularly preferred embodiment of the present invention; But those skilled in the art should recognize the effect of this embodiment and embodiment and only be used to set forth principle of the present invention, not constitute the restriction of the scope that the application is asked for protection.The useless bittern that the present invention discharges with Repone K production be a particularly preferred production process of the high-purity Magnesium dichloride hexahydrate of raw material production shown in accompanying drawing 1:
Useless bittern, sinking agent I and crystallization are carried out natural subsidence after selecting to reclaim the overflowing liquid uniform mixing; The clear liquid small portion is used for crystallization selection recovery circulation fluid after the sedimentation; Remaining clear liquid carries out the spontaneous evaporation crystallization, and crystallization control magnesium chloride amount is an original solution magnesium chloride total amount about 50%.The Magnesium dichloride hexahydrate coarse crystallization gathers out from the evaporative crystallization pond with the slurries form, carries out crystallization then and selects to reclaim, and the water-containing crystal of recovery obtains the coarse crystallization Magnesium dichloride hexahydrate through filtration, washing lotion washing.
Thick Magnesium dichloride hexahydrate is made near saturated solution with distilled water (or deionized water), and selects to reclaim the overflowing liquid uniform mixing in sinking agent II, secondary crystal, and subsequent process roughly with the evaporative crystallization treating processes is similar for the first time, repeats no more.The crystallization of wetting after filtering is carried out drying and is obtained finished product.
Below in conjunction with actual industrial processing instance treatment process is described further.
Used useless bittern in the industrial experiment, sinking agent, washing lotion situation are following:
Useless bittern composition actual measurement as follows (weight percent content, %):
MgCl
2 32.8 KCl 1.2
SO
4 2- 1.4 B 0.017
Fe 0.04 Ca 1.0
Mn 0.01 Sr 0.008
Br 0.01 Cr 0.02
After sinking agent I and sinking agent II were respectively one or more proportional mixing in AG hydrochloric acid, calcium chloride, bariumchloride, sodium-chlor, yellow soda ash, sodium hydroxide, polyoxyethylene glycol, polyacrylamide, the only son's acid, using distilled water to be mixed with percentage concentration was 10% and 5% solution.
Washing lotion preparation water adopts steam condensate, adds high-purity magnesium chloride hexahydrate finished product configuration dissolving of 1.1 times of theoretical consumptions, adds the sinking agent II of entry and high pure magnesium chloride gross weight 1% simultaneously, after fully stirring, seals static 24 hours, and it is subsequent use to get supernatant liquid.
Industrial experiment instance one
Useless bittern 5000Kg, sinking agent I 50Kg mixed 20 minutes, and continuously through settling bowl, 120 seconds settling bowl residence time, clear liquid 1000Kg gives over to crystallization and selects to reclaim circulation fluid after the sedimentation, the outer evaporation tank of all the other inlet chambers.After 3 days, evaporate total liquor capacity 14%, slurry is collected put into the buffering slurry tank then, send crystallization continuously to through spiral conveyer and select accumulator tank.Wherein, it is 0.3 meter per second through orifice plate V-bar that the accumulator tank circulation fluid is selected in crystallization, and the orifice plate aperture is 4 millimeters, percentage of open area 72%.The slurry that reclaims carries out continous vacuum and filters and wash, operation vacuum tightness 0.07MPa.Thereby obtain coarse crystallization 1200Kg.
In coarse crystallization, add steam condensate 400Kg, sinking agent II 16Kg, stirred 20 minutes, continuously through settling bowl, 120 seconds settling bowl residence time, clear liquid 520Kg gives over to secondary crystal and selects to reclaim circulation fluid after the sedimentation, the outer evaporation tank of all the other inlet chambers.After 3 days, evaporate total liquor capacity 17%, slurry is collected put into the buffering slurry tank then, send secondary crystal continuously to through spiral conveyer and select accumulator tank.Wherein, it is 0.3 meter per second through orifice plate V-bar that the accumulator tank circulation fluid is selected in crystallization, and the orifice plate aperture is 4 millimeters, percentage of open area 72%.The slurry of secondary recovery carries out continous vacuum and filters and wash, operation vacuum tightness 0.07MPa.Thereby obtain wet crystallization 440Kg, dried finished products 410Kg.
The check analysis result is following:
MgCl
2 46.64 KCl 0.001
SO
4 2- 3ppm B 2ppm
Fe 2ppm Ca 21ppm
Mn does not detect Sr and does not detect
Br 4ppm Cr does not detect
Industrial experiment instance two
Be with instance one difference; Crystallization for the first time selects to reclaim overflowing liquid in useless bittern and the instance one, sinking agent I mixes, and coarse crystallization and steam condensate, the crystallization for the second time that the first time, recrystallization obtained selects to reclaim overflowing liquid, sinking agent II mixes.All the other processes and operational condition and instance one are basic identical.Obtain finished product 510Kg after the final drying.
Two finished product composition analysis results are following for instance:
MgCl
2 46.60 KCl 0.002
SO
4 2- 4ppm ?B 3ppm
Fe 2ppm Ca 32ppm
Mn does not detect Sr and does not detect
Br 2ppm Cr does not detect
Industrial experiment is the result show, the treatment process that the present invention proposes is pratical and feasible, and the final product quality index can satisfy the Magnesium Chloride Anhydrous of electrolytic metal magnesium or the specification of quality of fire retardant magnesium hydroxide desired raw material.
Claims (10)
1. a useless bittern of discharging with Repone K production is the method for the high-purity magnesium chloride hexahydrate of raw material production, comprises the steps:
First purification phase comprises that useless bittern obtains coarse crystallization through first settling process, first evaporation and crystal process, first crystallization selection removal process, first filtration washing successively;
Second purification phase comprises resulting coarse crystallization is dissolved once more, selected removal process, the second filtration washing process through second settling process, second evaporation and crystal process, second crystallization, obtains wet crystallization, obtains finished product behind the crystallizing and drying that will wet;
It is characterized in that; Said first crystallization is selected to reclaim and second crystallization selects recovery to adopt crystallization to select withdrawer to come the crystallization of selective recovery certain grain size scope; Said crystallization selects withdrawer to have following structure: the opening for feed of crystallization withdrawer is arranged on the middle and upper part; The inclination sieve plate is equipped with in the opening for feed below; Be the circulating clear liquid import below the sieve plate, discharge port is arranged at the bottom; Wait that selecting to reclaim crystallization gets into from the withdrawer middle and upper part with the slurries form; Particle diameter is stopped entering macrobead recovery approach greater than 4 millimeters crystalline particle by sieve plate, reclaims or dissolve the back once more with coarse crystallization as byproduct to get into second purification phase; Diameter overflows withdrawer less than 0.1 millimeter particle with the current overflowing liquid that makes progress, and diameter 0.1-4 mm granules is deposited to the withdrawer bottom through the inclination sieve plate, is discharged by the bottom discharge mouth, gets into filtration washing process subsequently.
2. method according to claim 1 is characterized in that: in said first and/or second settling process, add sinking agent, the sinking agent that adds in said first and second settling processes can be identical or different.
3. method according to claim 2 is characterized in that, said sinking agent is selected from one or more the aqueous solution in AG hydrochloric acid, calcium chloride, bariumchloride, sodium-chlor, yellow soda ash, sodium hydroxide, polyoxyethylene glycol, polyacrylamide, the only son's acid.
4. method according to claim 3, sinking agent solution adopt distilled water or ultrapure water preparation, and the mass percent concentration of sinking agent solution is the solution of 1-25%.
5. method according to claim 4, the sinking agent solution usage is for needing the former liquid measure 0.5%-1.0% of sedimentation (weight).
6. according to the arbitrary described method of claim 1-5, it is characterized in that: said first evaporative crystallization and/or second evaporative crystallization adopt the spontaneous evaporation crystallization processes.
7. according to the arbitrary described method of claim 1-6, its characteristic is that also the washing lotion that the said first filtration washing process is used is the saturated magnesium chloride solution of steam condensate, distilled water, deionized water or the configuration of high-purity finished product magnesium chloride; The washing lotion of using in the perhaps said second filtration washing process is the saturated magnesium chloride solution of steam condensate and the configuration of high-purity finished product magnesium chloride; More preferably, the washing lotion of first, second filtration washing is the clear liquid of magnesium chloride saturated solution after sedimentation with steam condensate and finished product configuration; Preferred washing lotion consumption is the 10-30% of slurry weight.
8. according to the arbitrary described method of claim 1-7, it is characterized in that said coarse crystallization is dissolved the employing steam condensate once more.
9. according to the arbitrary described method of claim 1-8, it is characterized in that: the circulating clear liquid in first and second crystallizations selection removal process is respectively from clear liquid after the first time, the sedimentation for the second time.
10. according to the arbitrary described method of claim 1-8, it is characterized in that: first and second crystallizations select the current overflowing liquid in the removal process to mix with the solution after useless bittern, the coarse crystallization dissolving respectively, carry out subsequent sedimentation then and handle.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102452676A (en) * | 2010-10-26 | 2012-05-16 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| CN103991884A (en) * | 2014-05-27 | 2014-08-20 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride from low-grade sulfate subtype potassium tailings |
| CN104556187A (en) * | 2014-12-24 | 2015-04-29 | 湖北石花友谊化工股份有限公司 | Preparing technology of high-purity barium chloride |
| CN104628018A (en) * | 2013-11-15 | 2015-05-20 | 中国科学院过程工程研究所 | Methods for preparing magnesium chloride hexahydrate for producing electrolytic magnesium |
| CN106745112A (en) * | 2016-12-15 | 2017-05-31 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
| CN106917108A (en) * | 2017-03-20 | 2017-07-04 | 青海盐湖工业股份有限公司 | A kind of production technology of magnesium metal |
| CN110342553A (en) * | 2019-07-24 | 2019-10-18 | 武汉工程大学 | A kind of assisting crystallisation is evaporated brine the method for reducing Mg/Li ratio in salt lake |
| CN112723397A (en) * | 2020-12-16 | 2021-04-30 | 营口市荣兴达科技实业股份有限公司 | Composite refining technology for bischofite in salt lake |
| CN115321565A (en) * | 2022-08-03 | 2022-11-11 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing nano magnesium hydroxide by taking salt lake brine as raw material |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102452676A (en) * | 2010-10-26 | 2012-05-16 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| CN102452676B (en) * | 2010-10-26 | 2014-04-23 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| CN104628018A (en) * | 2013-11-15 | 2015-05-20 | 中国科学院过程工程研究所 | Methods for preparing magnesium chloride hexahydrate for producing electrolytic magnesium |
| CN103991884A (en) * | 2014-05-27 | 2014-08-20 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride from low-grade sulfate subtype potassium tailings |
| CN103991884B (en) * | 2014-05-27 | 2016-01-20 | 中国科学院青海盐湖研究所 | From low-grade vitriol hypotype containing the method preparing Repone K potassium mine tailing |
| CN104556187A (en) * | 2014-12-24 | 2015-04-29 | 湖北石花友谊化工股份有限公司 | Preparing technology of high-purity barium chloride |
| CN106745112A (en) * | 2016-12-15 | 2017-05-31 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
| CN106745112B (en) * | 2016-12-15 | 2018-04-06 | 河南豫辰药业股份有限公司 | The preparation method of Magnesium dichloride hexahydrate is reclaimed in a kind of waste residue hydrolyzate from grignard |
| CN106917108A (en) * | 2017-03-20 | 2017-07-04 | 青海盐湖工业股份有限公司 | A kind of production technology of magnesium metal |
| CN110342553A (en) * | 2019-07-24 | 2019-10-18 | 武汉工程大学 | A kind of assisting crystallisation is evaporated brine the method for reducing Mg/Li ratio in salt lake |
| CN110342553B (en) * | 2019-07-24 | 2022-04-29 | 武汉工程大学 | Method for reducing magnesium-lithium ratio in salt lake by auxiliary crystallization and salt drying |
| CN112723397A (en) * | 2020-12-16 | 2021-04-30 | 营口市荣兴达科技实业股份有限公司 | Composite refining technology for bischofite in salt lake |
| CN115321565A (en) * | 2022-08-03 | 2022-11-11 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing nano magnesium hydroxide by taking salt lake brine as raw material |
| CN115321565B (en) * | 2022-08-03 | 2023-10-13 | 国投新疆罗布泊钾盐有限责任公司 | Method for preparing nano magnesium hydroxide by taking salt lake brine as raw material |
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Application publication date: 20120208 |